CN107892320A - A kind of method that precipitated calcium carbonate is prepared with oyster shell whiting - Google Patents

A kind of method that precipitated calcium carbonate is prepared with oyster shell whiting Download PDF

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Publication number
CN107892320A
CN107892320A CN201711345865.1A CN201711345865A CN107892320A CN 107892320 A CN107892320 A CN 107892320A CN 201711345865 A CN201711345865 A CN 201711345865A CN 107892320 A CN107892320 A CN 107892320A
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calcium carbonate
oyster shell
parts
shell whiting
precipitated calcium
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黄浩
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Liuzhou Jihui Mechanical Design Co Ltd
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Liuzhou Jihui Mechanical Design Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/06—Washing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Abstract

The invention discloses a kind of method that precipitated calcium carbonate is prepared with oyster shell whiting, comprise the following steps：(1) oyster shell whiting pre-processes：Oyster shell whiting and deionized water are put into reactor, add acetic acid, then heat up, filter, filter residue is put rapidly into 5 DEG C of environment refrigerate it is standby；(2) it is calcined；(3) it is carbonized：Lime powder and deionized water are put into carbonization reactor, the packed sack for having porous silica titanium catalyst is put into deionized water, carbon dioxide is passed through under conditions of being 40~50 DEG C in ultrasonication, temperature to be carbonized, the pressure for keeping reaction system is 2~4MPa, after reacting 45min, obtained sediment is calcium carbonate crystal, after calcium carbonate crystal is carried out into heated-air drying processing, obtains precipitated calcium carbonate finished product.Precipitated calcium carbonate is prepared with wide material sources, cheap oyster shell whiting in the present invention, and the purity of the precipitated calcium carbonate prepared is high, can be widely applied to medicine, building decoration field.

Description

A kind of method that precipitated calcium carbonate is prepared with oyster shell whiting
【Technical field】
The invention belongs to the recovery field of shell, more particularly to a kind of method that precipitated calcium carbonate is prepared with oyster shell whiting.
【Background technology】
Precipitated calcium carbonate is a kind of extremely wide inorganic filler of purposes, and the output of current national precipitated calcium carbonate is Reach 400,000 tons/year.With the rapid development of the national economy, its demand still locates ascendant trend, especially construction industry in recent years By national requirements by plastic-steel door window, drainage pipeline to mould Dai Gang, while the popularization of paper industry alkaline bleach liquor sizing technology and Popularization and the increase of foreign export amount etc., more expand the application market of precipitated calcium carbonate.In terms of national market, precipitated calcium carbonate It is even more increasingly still in the state that supply falls short of demand, the especially demand of the precipitated calcium carbonate required for some special quality materials Increase.Analysis shows, particularly rubber, plastics, ink, papermaking processing manufacturing industry level are higher, to the demand of precipitated calcium carbonate Larger and quality requirement is high.
Oyster shell whiting is oyster shell whiting pulverized powder, and its 95% main component is calcium carbonate, also a small amount of amino acid and polysaccharide Material.The high-grade material of food, cosmetics and interior decoration can be done, it is widely applicable to animal and fowl fodder and food calcium source adds Add agent, ornaments processing, drier etc..It is one of new application of oyster shell whiting that oyster shell whiting, which prepares calcium carbonate, and natural environmental protection is that it is most heavy The advantage wanted.It is light for being prepared into but existing oyster shell whiting mainly prepares powdered whiting during preparing calcium carbonate The research of matter calcium carbonate is less.Therefore, research is a kind of prepares recovery profit of the method for precipitated calcium carbonate for shell with oyster shell whiting With with huge reference value.
【The content of the invention】
Present invention aims at a kind of method that precipitated calcium carbonate is prepared with oyster shell whiting is provided, the present invention first enters to oyster shell whiting Row pretreatment, the amino acid in oyster shell whiting and polysaccharide are removed；Then oyster shell whiting is calcined, generates calcium oxide；Finally exist It is carbonized under the catalytic action of porous silica titanium catalyst, obtains precipitated calcium carbonate.With wide material sources, price in the present invention Cheap oyster shell whiting prepares precipitated calcium carbonate, and the purity of the precipitated calcium carbonate prepared is high, can be widely applied to medicine, building dress Pool field.
To reach above-mentioned purpose, the technical solution adopted in the present invention is：It is a kind of to prepare precipitated calcium carbonate with oyster shell whiting Method, comprise the following steps：
(1) oyster shell whiting pre-processes：Count in parts by weight, 200 parts of oyster shell whitings and 500 parts of deionized waters are put into reactor In, 2 parts of acetic acid are added, then heat to 45~50 DEG C, filtering, filter residue is put rapidly into 5 DEG C of environment and refrigerates standby, obtained Pretreated oyster shell whiting；
(2) it is calcined：Pretreated oyster shell whiting is put into Muffle furnace, with 50~65 DEG C/min speed be rapidly heated to By 700~1000 DEG C, 2h is calcined, obtains lime powder；
(3) it is carbonized：Count in parts by weight, 100 parts of lime powders and 5000 parts of deionized waters are put into carbonization reactor In, the packed sack for having porous silica titanium catalyst is put into deionized water, ultrasonication power be 1000~ 1500W, temperature are passed through carbon dioxide under conditions of being 40~50 DEG C and are carbonized, and reaction system is kept during carbonization Pressure be 2~4MPa, react 45min after, obtained sediment is calcium carbonate crystal, and calcium carbonate crystal is carried out into hot air drying After dry processing, precipitated calcium carbonate finished product is obtained.
In the present invention, as further explanation, the porous silica titanium catalyst described in step (3) is by following method systems It is standby：Count in parts by weight, 100 parts of ethanol solutions, 1 part of surfactant and 2 parts of ferric sulfate are put into reactor, start stirring Device, it is stirred in 200~500r/min speed, while 10 parts of butyl titanates is added with 2mL/min speed, is continued 2~3h is reacted, after vacuum distillation, is precipitated with absolute ethyl alcohol, collects sediment, and 25min is rinsed with pure water, is protected It is 30~50L/ (m to hold backwash rate2S), the sediment after flushing is placed on after Muffle furnace is calcined, obtained doped with iron The porous silica titanium catalyst of ion.
In the present invention, as further explanation, the mass fraction of described ethanol solution is 65~75%.
In the present invention, as further explanation, the oyster shell whiting described in step (1) is oyster shell powder, car spiral case powder or thorn Spiral case powder.
In the present invention, it is as further explanation, the parameter of the heated-air drying processing described in step (3)：Temperature is 115 ~130 DEG C, drying time be 6~10h.
In the present invention, as further explanation, the water content of the precipitated calcium carbonate finished product described in step (3) for 0.3~ 1%.
The function introduction of part material is as follows：
Acetic acid, while being used to soften oyster shell whiting in the present invention, it is dissolved in water, the amino in oyster shell whiting can be dissolved Acid and polysaccharide, reach the amino acid removed in oyster shell whiting, the purpose of polysaccharide.
Carbon dioxide, is used as in the present invention and calcium hydroxide reaction generates precipitation of calcium carbonate.
Ethanol solution, it is used as the reactant for preparing porous silica titanium catalyst in the present invention, for dissolving metatitanic acid four Butyl ester.
Ferric sulfate, in the present invention in be used as the main reactant for preparing porous silica titanium catalyst, for providing iron Ion.
Butyl titanate, it is used as being used as the key reaction for preparing porous silica titanium catalyst in preparing in the present invention Thing, as titanium source.
The invention has the advantages that：
1. technological means of the present invention employed in carbonisation can shorten the same of time for preparing precipitated calcium carbonate When, improve the purity of precipitated calcium carbonate.The present invention first makes calcium oxide and water generate calcium hydroxide precipitation in carbonisation；So Add the porous silica titanium catalyst doped with iron ion afterwards, by under the catalytic action of iron ion, make calcium hydroxide and Carbon dioxide contacts rapidly, then aids in the treatment conditions with ultrasonic wave, calcium hydroxide is constantly vibrated and is disperseed, and further increases With the contact area of carbon dioxide, and then generate high-purity precipitated calcium carbonate.Each technological means of the present invention is mutual Coordinate, mutually promote, be indispensable, the total effect reached is significantly larger than the simple of the effect acquired by single technological means Add and.
2. it is titanium doped to have started porous silica doped with iron ion for the porous silica C catalyst prepared by the present invention The new tool of metal ion.The present invention uses sol-gel process, using ferric sulfate as Doped ions presoma, in the environment of ethanol Under be stirred, while be slowly added to the titanium source of butyl titanate, after alcohol precipitation, roasting, obtain doped with the more of iron ion Porous titanium dioxide catalyst.
2. the technological means of oyster shell whiting pretreatment of the present invention can efficiently remove polysaccharide and ammonia in oyster shell whiting Base acid, the content of calcium carbonate in oyster shell whiting is improved, and then the preparation for follow-up lifting high-purity precipitated calcium carbonate hides the foreshadowing.
【Embodiment】
Embodiment 1：
1. early-stage preparations
The preparation of porous silica titanium catalyst：Count in parts by weight, 100 parts of mass fractions are molten for 65% ethanol Liquid, 1 part of surfactant and 2 parts of ferric sulfate are put into reactor, are started agitating device, are stirred in 200r/min speed Mix, while 10 parts of butyl titanates are added with 2mL/min speed, continue to react 2h, after vacuum distillation, use absolute ethyl alcohol Precipitated, collect sediment, and 25min is rinsed with pure water, holding backwash rate is 30L/ (m2S), by after flushing Sediment is placed on after Muffle furnace is calcined, and obtains the porous silica titanium catalyst doped with iron ion.
Above-mentioned prepared material is used in following preparation methods.
2. a kind of method that precipitated calcium carbonate is prepared with oyster shell whiting, comprises the following steps：
(1) oyster shell whiting pre-processes：Count in parts by weight, 200 parts of oyster shell powders and 500 parts of deionized waters are put into reactor In, 2 parts of acetic acid are added, then heat to 45 DEG C, filtering, filter residue is put rapidly into 5 DEG C of environment and refrigerates standby, obtain pre- place Oyster shell whiting after reason；
(2) it is calcined：Pretreated oyster shell whiting is put into Muffle furnace, is rapidly heated with 50 DEG C/min speed to general 700 DEG C, 2h is calcined, obtains lime powder；
(3) it is carbonized：Count in parts by weight, 100 parts of lime powders and 5000 parts of deionized waters are put into carbonization reactor In, the packed sack for having porous silica titanium catalyst is put into deionized water, is 1000W, temperature in ultrasonication power Spend and be carbonized to be passed through carbon dioxide under conditions of 40 DEG C, the pressure that reaction system is kept during carbonization is 2MPa, react 45min after, obtained sediment is calcium carbonate crystal, by calcium carbonate crystal at 115 DEG C heated-air drying 6h Afterwards, the precipitated calcium carbonate finished product that water content is 1% is obtained.
After testing, the purity of precipitated calcium carbonate is 99.99%.
Embodiment 2：
1. early-stage preparations
The preparation of porous silica titanium catalyst：Count in parts by weight, 100 parts of mass fractions are molten for 68% ethanol Liquid, 1 part of surfactant and 2 parts of ferric sulfate are put into reactor, are started agitating device, are stirred in 300r/min speed Mix, while 10 parts of butyl titanates are added with 2mL/min speed, continue to react 2.5h, after vacuum distillation, with anhydrous second Alcohol is precipitated, and collects sediment, and rinses 25min with pure water, and holding backwash rate is 37L/ (m2S), by after flushing Sediment be placed on after Muffle furnace is calcined, obtain the porous silica titanium catalyst doped with iron ion.
Above-mentioned prepared material is used in following preparation methods.
2. a kind of method that precipitated calcium carbonate is prepared with oyster shell whiting, comprises the following steps：
(1) oyster shell whiting pre-processes：Count in parts by weight, 200 parts of car spiral case powder and 500 parts of deionized waters are put into reactor In, 2 parts of acetic acid are added, then heat to 46 DEG C, filtering, filter residue is put rapidly into 5 DEG C of environment and refrigerates standby, obtain pre- place Oyster shell whiting after reason；
(2) it is calcined：Pretreated oyster shell whiting is put into Muffle furnace, is rapidly heated with 55 DEG C/min speed to general 800 DEG C, 2h is calcined, obtains lime powder；
(3) it is carbonized：Count in parts by weight, 100 parts of lime powders and 5000 parts of deionized waters are put into carbonization reactor In, the packed sack for having porous silica titanium catalyst is put into deionized water, is 1100W, temperature in ultrasonication power Spend and be carbonized to be passed through carbon dioxide under conditions of 44 DEG C, the pressure that reaction system is kept during carbonization is 3MPa, react 45min after, obtained sediment is calcium carbonate crystal, by calcium carbonate crystal at 118 DEG C heated-air drying 8h Afterwards, the precipitated calcium carbonate finished product that water content is 0.6% is obtained.
After testing, the purity of precipitated calcium carbonate is 99.95%.
Embodiment 3：
1. early-stage preparations
The preparation of porous silica titanium catalyst：Count in parts by weight, 100 parts of mass fractions are molten for 70% ethanol Liquid, 1 part of surfactant and 2 parts of ferric sulfate are put into reactor, are started agitating device, are stirred in 400r/min speed Mix, while 10 parts of butyl titanates are added with 2mL/min speed, continue to react 2.5h, after vacuum distillation, with anhydrous second Alcohol is precipitated, and collects sediment, and rinses 25min with pure water, and holding backwash rate is 42L/ (m2S), by after flushing Sediment be placed on after Muffle furnace is calcined, obtain the porous silica titanium catalyst doped with iron ion.
Above-mentioned prepared material is used in following preparation methods.
2. a kind of method that precipitated calcium carbonate is prepared with oyster shell whiting, comprises the following steps：
(1) oyster shell whiting pre-processes：Count in parts by weight, 200 parts of thorn spiral case powder and 500 parts of deionized waters are put into reactor In, 2 parts of acetic acid are added, then heat to 48 DEG C, filtering, filter residue is put rapidly into 5 DEG C of environment and refrigerates standby, obtain pre- place Oyster shell whiting after reason；
(2) it is calcined：Pretreated oyster shell whiting is put into Muffle furnace, is rapidly heated with 60 DEG C/min speed to general 900 DEG C, 2h is calcined, obtains lime powder；
(3) it is carbonized：Count in parts by weight, 100 parts of lime powders and 5000 parts of deionized waters are put into carbonization reactor In, the packed sack for having porous silica titanium catalyst is put into deionized water, is 1400W, temperature in ultrasonication power Spend and be carbonized to be passed through carbon dioxide under conditions of 45 DEG C, the pressure that reaction system is kept during carbonization is 2.5MPa, react 45min after, obtained sediment is calcium carbonate crystal, by calcium carbonate crystal at 120 DEG C heated-air drying 9h Afterwards, the precipitated calcium carbonate finished product that water content is 0.5% is obtained.
After testing, the purity of precipitated calcium carbonate is 99.98%.
Embodiment 4：
1. early-stage preparations
The preparation of porous silica titanium catalyst：Count in parts by weight, 100 parts of mass fractions are molten for 70% ethanol Liquid, 1 part of surfactant and 2 parts of ferric sulfate are put into reactor, are started agitating device, are stirred in 350r/min speed Mix, while 10 parts of butyl titanates are added with 2mL/min speed, continue to react 3h, after vacuum distillation, use absolute ethyl alcohol Precipitated, collect sediment, and 25min is rinsed with pure water, holding backwash rate is 46L/ (m2S), by after flushing Sediment is placed on after Muffle furnace is calcined, and obtains the porous silica titanium catalyst doped with iron ion.
Above-mentioned prepared material is used in following preparation methods.
2. a kind of method that precipitated calcium carbonate is prepared with oyster shell whiting, comprises the following steps：
(1) oyster shell whiting pre-processes：Count in parts by weight, 200 parts of oyster shell powders and 500 parts of deionized waters are put into reactor In, 2 parts of acetic acid are added, then heat to 47 DEG C, filtering, filter residue is put rapidly into 5 DEG C of environment and refrigerates standby, obtain pre- place Oyster shell whiting after reason；
(2) it is calcined：Pretreated oyster shell whiting is put into Muffle furnace, is rapidly heated with 60 DEG C/min speed to general 850 DEG C, 2h is calcined, obtains lime powder；
(3) it is carbonized：Count in parts by weight, 100 parts of lime powders and 5000 parts of deionized waters are put into carbonization reactor In, the packed sack for having porous silica titanium catalyst is put into deionized water, is 1200W, temperature in ultrasonication power Spend and be carbonized to be passed through carbon dioxide under conditions of 43 DEG C, the pressure that reaction system is kept during carbonization is 3.5MPa, react 45min after, obtained sediment is calcium carbonate crystal, by calcium carbonate crystal at 125 DEG C heated-air drying 8h Afterwards, the precipitated calcium carbonate finished product that water content is 0.5% is obtained.
After testing, the purity of precipitated calcium carbonate is 99.99%.
Embodiment 5：
1. early-stage preparations
The preparation of porous silica titanium catalyst：Count in parts by weight, 100 parts of mass fractions are molten for 69% ethanol Liquid, 1 part of surfactant and 2 parts of ferric sulfate are put into reactor, are started agitating device, are stirred in 450r/min speed Mix, while 10 parts of butyl titanates are added with 2mL/min speed, continue to react 2.5h, after vacuum distillation, with anhydrous second Alcohol is precipitated, and collects sediment, and rinses 25min with pure water, and holding backwash rate is 42L/ (m2S), by after flushing Sediment be placed on after Muffle furnace is calcined, obtain the porous silica titanium catalyst doped with iron ion.
Above-mentioned prepared material is used in following preparation methods.
2. a kind of method that precipitated calcium carbonate is prepared with oyster shell whiting, comprises the following steps：
(1) oyster shell whiting pre-processes：Count in parts by weight, 200 parts of car spiral case powder and 500 parts of deionized waters are put into reactor In, 2 parts of acetic acid are added, then heat to 49 DEG C, filtering, filter residue is put rapidly into 5 DEG C of environment and refrigerates standby, obtain pre- place Oyster shell whiting after reason；
(2) it is calcined：Pretreated oyster shell whiting is put into Muffle furnace, is rapidly heated with 63 DEG C/min speed to general 900 DEG C, 2h is calcined, obtains lime powder；
(3) it is carbonized：Count in parts by weight, 100 parts of lime powders and 5000 parts of deionized waters are put into carbonization reactor In, the packed sack for having porous silica titanium catalyst is put into deionized water, is 1300W, temperature in ultrasonication power Spend and be carbonized to be passed through carbon dioxide under conditions of 47 DEG C, the pressure that reaction system is kept during carbonization is 3.5MPa, react 45min after, obtained sediment is calcium carbonate crystal, by calcium carbonate crystal at 120 DEG C heated-air drying 8h Afterwards, the precipitated calcium carbonate finished product that water content is 6% is obtained.
After testing, the purity of precipitated calcium carbonate is 99.98%.
Embodiment 6：
1. early-stage preparations
The preparation of porous silica titanium catalyst：Count in parts by weight, 100 parts of mass fractions are molten for 75% ethanol Liquid, 1 part of surfactant and 2 parts of ferric sulfate are put into reactor, are started agitating device, are stirred in 500r/min speed Mix, while 10 parts of butyl titanates are added with 2mL/min speed, continue to react 3h, after vacuum distillation, use absolute ethyl alcohol Precipitated, collect sediment, and 25min is rinsed with pure water, holding backwash rate is 50L/ (m2S), by after flushing Sediment is placed on after Muffle furnace is calcined, and obtains the porous silica titanium catalyst doped with iron ion.
Above-mentioned prepared material is used in following preparation methods.
2. a kind of method that precipitated calcium carbonate is prepared with oyster shell whiting, comprises the following steps：
(1) oyster shell whiting pre-processes：Count in parts by weight, 200 parts of thorn spiral case powder and 500 parts of deionized waters are put into reactor In, 2 parts of acetic acid are added, then heat to 50 DEG C, filtering, filter residue is put rapidly into 5 DEG C of environment and refrigerates standby, obtain pre- place Oyster shell whiting after reason；
(2) it is calcined：Pretreated oyster shell whiting is put into Muffle furnace, is rapidly heated with 65 DEG C/min speed to general 1000 DEG C, 2h is calcined, obtains lime powder；
(3) it is carbonized：Count in parts by weight, 100 parts of lime powders and 5000 parts of deionized waters are put into carbonization reactor In, the packed sack for having porous silica titanium catalyst is put into deionized water, is 1500W, temperature in ultrasonication power Spend and be carbonized to be passed through carbon dioxide under conditions of 50 DEG C, the pressure that reaction system is kept during carbonization is 4MPa, react 45min after, obtained sediment is calcium carbonate crystal, by calcium carbonate crystal at 130 DEG C heated-air drying 10h Afterwards, the precipitated calcium carbonate finished product that water content is 0.3% is obtained.
After testing, the purity of precipitated calcium carbonate is 99.99%.
Described above is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair Bright patent claim, the equal change completed or modification change under the technical spirit suggested by all present invention, all should belong to Cover the scope of the claims in the present invention.

Claims (6)

  1. A kind of 1. method that precipitated calcium carbonate is prepared with oyster shell whiting, it is characterised in that：Comprise the following steps：
    (1) oyster shell whiting pre-processes：Count in parts by weight, 200 parts of oyster shell whitings and 500 parts of deionized waters are put into reactor, added Enter 2 parts of acetic acid, then heat to 45~50 DEG C, filtering, filter residue is put rapidly into 5 DEG C of environment and refrigerate standby, obtain pre- place Oyster shell whiting after reason；
    (2) it is calcined：Pretreated oyster shell whiting is put into Muffle furnace, is rapidly heated with 50~65 DEG C/min speed to general 700~1000 DEG C, 2h is calcined, obtains lime powder；
    (3) it is carbonized：Count in parts by weight, 100 parts of lime powders and 5000 parts of deionized waters are put into carbonization reactor, will The packed sack for having porous silica titanium catalyst is put into deionized water, is 1000~1500W, temperature in ultrasonication power Spend and be carbonized to be passed through carbon dioxide under conditions of 40~50 DEG C, the pressure that reaction system is kept during carbonization is 2~4MPa, after reacting 45min, obtained sediment is calcium carbonate crystal, and calcium carbonate crystal is carried out into heated-air drying processing Afterwards, precipitated calcium carbonate finished product is obtained.
  2. A kind of 2. method that precipitated calcium carbonate is prepared with oyster shell whiting according to claim 1, it is characterised in that：Step (3) Described porous silica titanium catalyst is prepared by following methods：Count in parts by weight, 100 parts of ethanol solutions, 1 part of surface are lived Property agent and 2 parts of ferric sulfate be put into reactor, start agitating device, be stirred in 200~500r/min speed, at the same with 2mL/min speed adds 10 parts of butyl titanates, continues 2~3h of reaction, after vacuum distillation, is sunk with absolute ethyl alcohol Form sediment, collect sediment, and 25min is rinsed with pure water, holding backwash rate is 30~50L/ (m2S), will be heavy after flushing Starch is placed on after Muffle furnace is calcined, and obtains the porous silica titanium catalyst doped with iron ion.
  3. A kind of 3. method that precipitated calcium carbonate is prepared with oyster shell whiting according to claim 2, it is characterised in that：Described second The mass fraction of alcoholic solution is 65~75%.
  4. A kind of 4. method that precipitated calcium carbonate is prepared with oyster shell whiting according to claim 1, it is characterised in that：Step (1) Described oyster shell whiting is oyster shell powder, car spiral case powder or thorn spiral case powder.
  5. A kind of 5. method that precipitated calcium carbonate is prepared with oyster shell whiting according to claim 1, it is characterised in that：Step (3) The parameter of described heated-air drying processing is：Temperature is 115~130 DEG C, drying time is 6~10h.
  6. A kind of 6. method that precipitated calcium carbonate is prepared with oyster shell whiting according to claim 1, it is characterised in that：Step (3) The water content of described precipitated calcium carbonate finished product is 0.3~1%.
CN201711345865.1A 2017-12-15 2017-12-15 A kind of method that precipitated calcium carbonate is prepared with oyster shell whiting Withdrawn CN107892320A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108975373A (en) * 2018-08-09 2018-12-11 天津中科福源科技有限责任公司 A method of precipitated calcium carbonate is prepared with conch meal
CN110115690A (en) * 2019-05-14 2019-08-13 五邑大学 A kind of toothpaste and preparation method thereof
CN115231600A (en) * 2022-07-25 2022-10-25 宁远华创粉体材料有限公司 Preparation method of suspended nano calcium carbonate for food

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108975373A (en) * 2018-08-09 2018-12-11 天津中科福源科技有限责任公司 A method of precipitated calcium carbonate is prepared with conch meal
CN110115690A (en) * 2019-05-14 2019-08-13 五邑大学 A kind of toothpaste and preparation method thereof
CN115231600A (en) * 2022-07-25 2022-10-25 宁远华创粉体材料有限公司 Preparation method of suspended nano calcium carbonate for food

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Application publication date: 20180410